Gas chromatography/mass spectrometry method for the quantitation of 3-chloro-p-toluidine hydrochloride in birds using a deuterated surrogate
1998
Hurlbut, D.B. | Johnston, J.J. | Daniel, S.R. | Tawara, J.
A method was developed for the quantitation of the avicide 3-chloro-p-toluidine hydrochloride (CPTH) in pigeon breast muscle and gastrointestinal tract. Accuracy and precision were greatly improved by the use of CPTH-d6 as a surrogate. CPTH-d6 was synthesized by the nitration of toluene-d8 followed by chlorination and reduction. The synthetic product provided mass fragments such that CPTH and the surrogate were differentiated by gas chromatography/mass spectrometry (GC/MS). A tissue extraction process used solid-phase extraction to concentrate the free base forms of CPTH and the surrogate from hexane extracts. These compounds were recovered from the SPE columns with n-butyl acetate and quantified by GC/MS. Validation data indicated (1) a linear relation between CPTH/CPTH-d6 area ratios and CPTH concentration; (2) a method limit of detection of 30 ppb for both tissue matrices; (3) CPTH recoveries from fortified tissues ranging from 56.4 to 92.4% whereas surrogate corrected recoveries ranged from 95.0 to 101%; and (4) identical extraction efficiencies of both compounds from each matrix.
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